US7353687B2 - Reference leak - Google Patents

Reference leak Download PDF

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Publication number
US7353687B2
US7353687B2 US11/228,821 US22882105A US7353687B2 US 7353687 B2 US7353687 B2 US 7353687B2 US 22882105 A US22882105 A US 22882105A US 7353687 B2 US7353687 B2 US 7353687B2
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Prior art keywords
leak
holes
diameter
gas
length
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US11/228,821
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US20060144120A1 (en
Inventor
Jie Tang
Liang Liu
Peng Liu
Zhao-Fu Hu
Bing-Chu Du
Cai-Lin Guo
Pi-Jin Chen
Shou-Shan Fan
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Tsinghua University
Hon Hai Precision Industry Co Ltd
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Tsinghua University
Hon Hai Precision Industry Co Ltd
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Assigned to TSINGHUA UNIVERSITY, HON HAI PRECISION INDUSTRY CO., LTD. reassignment TSINGHUA UNIVERSITY ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: LIU, PENG, CHEN, PI-JIN, DU, BING-CHU, FAN, SHOU-SHAN, GUO, CAI-LIN, HU, ZHAO-FU, LIU, LIANG, TANG, JIE
Publication of US20060144120A1 publication Critical patent/US20060144120A1/en
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M3/00—Investigating fluid-tightness of structures
    • G01M3/007—Leak detector calibration, standard leaks

Definitions

  • the present invention relates to detecting instruments for use in leak detection of a gas, particularly to a reference leak.
  • a reference leak is an artificial instrument for use in leak detection of a specific gas.
  • the reference leak has a constant leak rate for the specific gas under a given condition such as a specific temperature and a specific pressure at the gas intake side.
  • the reference leak has been widely used in periodical leak detection and calibration of a helium mass spectrometer leak detector.
  • a leak rate of the platinum wire-glass leak is generally in the range from 10 ⁇ 6 ⁇ 10 ⁇ 8 torr ⁇ l/s.
  • the platinum wire-glass leak is obtained by implanting a platinum wire into a glass body by way of a glass-to-metal unmatched sealing method. Due to a coefficient of thermal expansion of the platinum wire being unmatched with that of the glass body, a plurality of leak gaps are then defined at an interface between the platinum wire and the glass body. The platinum wire-glass leak is then obtained.
  • a leak rate of the reference leak has to be calibrated by other reference calibration instruments after the reference leak is manufactured. Additionally, the leak rate of the reference leak is sensitive to temperatures. The leak rate may vary due to a change of the number and distribution of the leak gaps as a result of a change of the temperature. This temperature dependence may cause uncertainties (i.e., potential for an increased margin of error) with respect to the leak rate of the platinum wire-glass leak.
  • the squeezed metal tube leak is generally obtained by punching a tube of an oxygen free copper into a flattened piece by a hydraulic pressure device.
  • the squeezed metal tube comprises a plurality of leak gaps, the leak gaps functioning as leak channels for the gas.
  • a leak rate of the squeezed metal tube type reference leak is generally in the range from 10 ⁇ 6 ⁇ 10 ⁇ 8 tor ⁇ l/s.
  • shapes, sizes, and numbers of the leak gaps of the squeezed metal tube leak are also formed randomly making such leak gaps unpredictable and therefore artificially uncontrollable.
  • the silica membrane helium leak is generally in a form of a blown bubble.
  • the blown bubble is generally a thin, spherical membrane formed of silica glass.
  • the silica glass membrane is porus and allows helium (He) gas to pass therethrough while blocking other kinds of gases from passing therethrough.
  • He helium
  • a leak rate of such a reference leak is unpredictable and has to be calibrated by other reference calibration instruments.
  • the leak rate of the reference leak is also sensitive to temperatures.
  • a method for making a reference leak comprises the steps of: (a) preparing a substrate; (b) forming a patterned catalyst layer on the substrate, the patterned catalyst layer comprising one or more catalyst blocks; (c) forming one or more predominantly one-dimensional, elongated nano-structures extending from the corresponding catalyst blocks, such elongate nano-structures being formed by a chemical vapor deposition method; (d) forming a leak layer of one of a metallic material, a glass material, and a ceramic material on the substrate, the one or more elongate nano-structures being partly or completely embedded in the leak layer; and (e) removing the one or more elongate nano-structures and the substrate to obtain a reference leak with one or more leak holes defined therein.
  • the substrate may be a silicon substrate.
  • a crystal plane orientation of the silicon may be selected from the group consisting of (111), (110), and (100) crystal plane orientations.
  • the patterned catalyst layer generally comprises a material selected from the group consisting of gold, iron, cobalt, and silver.
  • a thickness of the patterned catalyst layer is generally in the range from 0.2 nm to 10 nm.
  • the thickness of the patterned catalyst layer is preferably approximately 1 nm.
  • a size (i.e., diameter) of the catalyst block is preferably less than 1 ⁇ m.
  • the catalyst layer may be formed by an evaporation deposition method, a sputtering deposition method, or an electroplating method.
  • the catalyst layer may be patterned by a photolithography method or by an electron beam etching method.
  • the patterned catalyst layer may also be formed by a printing method.
  • the elongate nano-structures are, advantageously, generally selected from the group consisting of silicon nanowires, silicon dioxide nanowires, gallium nitride nanowires, indium phosphide nanowires, and zinc oxide nanowires.
  • a length of the elongate nano-structure is generally in the range from 100 nm to 100 ⁇ m.
  • a diameter or width of the elongate nano-structure is generally in the range from 10 nm to 500 nm.
  • the metallic material used for the leak layer may, advantageously, be selected from the group consisting of copper, nickel, and molybdenum, and alloys composed substantially of one or more of these metals.
  • the leak layer may be formed, e.g., by one of an evaporation deposition method, a sputtering deposition method, an electroplating method, a chemical vapor deposition method and a metal organic chemical vapor deposition method.
  • the one or more elongate nano-structures may later be effectively removed by one of a reactive ion etching method, a wet etching and a plasma etching method, for example.
  • a method for making a reference leak having a custom-tailored leak rate for use in leak detection of a gas includes the steps of:
  • a length of each of the elongate nano-structures is preferably not less than 20 times a diameter thereof.
  • a method for making a reference leak comprises the steps of: (a) forming one or more elongate nano-structures on a substrate; (b) forming a leak layer of one of a metallic material, a glass material, a composite material, and a ceramic material on the substrate with the one or more elongate nano-structures partly or completely embedded therein; and (c) removing the one or more elongate nano-structures and the substrate to obtain a reference leak with one or more corresponding leak holes defined therein.
  • FIGS. 1-5 are schematic, cross-sectional views showing successive stages in a method for making a reference leak, according to an exemplary embodiment of the present invention.
  • FIG. 6 is a schematic cross-sectional view showing the reference leak according to a preferred embodiment of the present invention.
  • the reference leak 100 comprises a leak layer 30 , and a plurality of leak through holes 301 defined in the leak layer 30 .
  • the leak layer 30 is, advantageously, generally formed of one of a metallic material, a glass material, a composite material, and a ceramic material.
  • the metallic material if chosen, may usefully be selected from the group consisting of copper, nickel, and molybdenum, and alloys composed substantially of at least one of such metals.
  • the material of the leak layer 30 is selected depending on the specific kind of a gas which the reference leak is utilized to detect. For instance, if the reference leak 100 is utilized to detect He gas, the material of the leak layer 30 is preferably a metallic material, because the metallic material is impermeable to He gas.
  • the material of the leak layer 30 is preferably a glass material or a ceramic material, because the glass material and the ceramic material are impermeable to air, O 2 gas, and/or Ar gas.
  • the leak through holes 301 may be shaped as cylindrical holes or polyhedral holes.
  • the number of the leak through holes 301 may be custom-tailored. In other words, the number of the leak through holes 301 may be predetermined prior to making the reference leak 100 .
  • the leak through holes 301 have substantially same length L and diameter D, and are substantially parallel to each other.
  • a shape, a length, and a diameter of each of the leak through holes 301 may also be custom-tailored and, thereby, predetermined prior to making the reference leak 100 .
  • the length L and the diameter D of each of the leak through holes preferably satisfy the following requirement: L ⁇ 20 D.
  • the diameter of each of the leak through holes 301 is generally in the range from 10 nm to 500 nm.
  • the length of each of the leak through holes 301 is generally in the range from 100 nm to 100 ⁇ m.
  • a leak rate of the reference leak 100 is generally in the range from 10 ⁇ 15 to 10 ⁇ 18 tor ⁇ l/s.
  • the reference leak 100 can be employed, for example, in leak detection and calibration of a helium mass spectrometer, in measurement of pumping speed of micro vacuum pump, and in supplying a mircoflow gas in experiments in the field of gas-solid interface technology.
  • FIGS. 1-5 the process for making a reference leak 10 according to a preferred embodiment of the present invention is shown.
  • the process includes the steps of:
  • a diameter and a length of each of the one or more elongate nano-structures 11 can be predetermined according to the given custom-tailored leak rate, which will be explained in detail below.
  • a substrate 1 is prepared.
  • the substrate 1 generally is a silicon substrate.
  • a crystal plane orientation of the silicon substrate 3 is advantageously selected from the group consisting of (111), (110), and (100) crystal plane orientations.
  • the crystal plane orientation of the silicone substrate is a (111) crystal plane orientation.
  • a catalyst layer 2 is formed on the substrate 1 by, e.g., an evaporation deposition method, a sputtering deposition method, or an electroplating method.
  • the catalyst layer 2 generally is composed of a material selected from the group consisting of gold, iron, cobalt, and silver, or an alloy composed substantially of least one of such metals.
  • the catalyst layer 2 is a layer of gold.
  • the catalyst layer 2 is then patterned, for example, by a photolithography method or an electron beam etching method. Alternatively, the patterned catalyst layer is formed by a printing method. A thickness of the patterned catalyst layer 2 is generally in the range from 0.2 nm to 10 nm.
  • the thickness of the patterned catalyst layer is approximately 1 nm.
  • the patterned catalyst layer 2 includes one or more catalyst blocks 21 .
  • Each catalyst particle 21 is located at a respective chosen site at which a given elongate nano-structure 11 is desired to be formed.
  • a size of the catalyst block 21 is preferably less than 1 ⁇ m.
  • Each of the catalyst blocks 21 is transformed into a single catalyst particle in a later growth process with only one elongate nano-structure 11 (see FIG. 3 ) being grown therefrom.
  • a shape of the catalyst particle 21 may be round or polygonal.
  • the treated substrate 1 together with the catalyst particles 21 , is placed in a reactive chamber (not shown) for performing a chemical vapor deposition (CVD) method.
  • a gas containing silicon for example, a SiCl 4 gas
  • a temperature in the reactive chamber is elevated and maintained in the range from 700° C. to 900° C.
  • one or more elongate nano-structures 11 are thus formed extending from the corresponding catalyst particles 21 .
  • the elongate nano-structures 11 are silicon nanowires 11 .
  • the silicon nanowires 11 are cylindrical and extend perpendicularly from the substrate 1 .
  • the length and the diameter of the silicon nanowire 11 can be artificially controlled by deliberately adjusting the thickness of the catalyst layer 2 , the concentration of ambient air, the growing temperature, and the growing time of the silicon nanowires 11 , etc.
  • the elongate nano-structures 11 may also, for example, be selected from the group consisting of silicon dioxide nanowires, gallium nitride nanowires, indium phosphide nanowires, and zinc oxide nanowires.
  • a length of the elongate nano-structure 11 is generally in the range from 100 nm to 100 ⁇ m.
  • a diameter (the term being intended to broadly incorporate width, if polyhedral in cross-section, as well as the standard meaning of “diameter” to simplify terminology) of the elongate nano-structure 11 is in the range from 10 nm to 500 nm.
  • the length and the diameter of the elongate nano-structure 11 may also be artificially controlled by deliberately adjusting the size of the catalyst particle 21 , the concentration of ambient air, the growing temperature, and the growing time of the elongate nano-structures 11 .
  • the silicon nanowires 11 are preferably oxidized into silicon dioxide nanowires 11 .
  • the length of the silicon nanowires 11 is preferably 20 times the diameter thereof, for ensuring that an error of a leak rate of the resultant reference leak is less than about 5%. (It is to be understood, that while CVD may be the current preferred method for forming nano-structures 11 , other deposition techniques may be employed for the formation of such nano-structures 11 and still be considered to be within the scope of the present invention.)
  • a leak layer 3 is formed on the substrate 1 with the one or more elongate nano-structures 11 partly or completely embedded therein.
  • the leak layer 3 may be formed, e.g., by an evaporation deposition method, a sputtering deposition method, an electroplating method, a chemical vapor deposition method and/or a metal organic chemical vapor deposition method.
  • the leak layer 3 may comprise a metallic material, a glass material, a composite material, or a ceramic material.
  • the material of the leak layer 30 is selected depending on the specific kind of a gas that the reference leak 10 is utilized to detect.
  • the leak layer 3 is comprised of a metallic material, such as copper, nickel, and molybdenum, or an alloy thereof.
  • a top portion of the leak layer 3 may be trimmed mechanically or by an electrochemical polishing process such that tip portions of the trimmed silicon nanowires 11 are flush with a top portion of the trimmed leak layer 3 , with the length of the silicon nanowires 11 still being maintained so as to be at least 20 times the diameter thereof.
  • step (c) referring to FIG. 5 , the one or more elongate nano-structures 11 , i.e., the silicon nanowires 11 , and the substrate 1 are then removed to obtain a reference leak 10 with one or more leak holes 31 defined therein.
  • the silicon nanowires 11 and the substrate 1 are removed by a reactive ion etching method, while the leak layer 3 (i.e. the metallic layer 3 ) remains intact.
  • the one or more elongate nano-structures 11 may be removed by a wet etching or a plasma etching method.
  • each of the leak through holes 31 has a same diameter as the silicon nanowires 11 .
  • the length of each of the leak through holes is equal to the length of the silicon nanowires 11 .
  • the number of the leak through holes 31 is equal to the number of the silicon nanowires 11 .
  • the leak through holes 31 extend perpendicularly from the substrate 1 and are parallel to each other.
  • the leak rate Q of the reference leak 10 can be predetermined according to the aforementioned equations prior to making the reference leak 10 .

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Examining Or Testing Airtightness (AREA)
US11/228,821 2005-01-06 2005-09-16 Reference leak Active 2025-10-17 US7353687B2 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CNB2005100327315A CN100462706C (zh) 2005-01-06 2005-01-06 标准漏孔
CN200510032731.5 2005-01-06

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060143895A1 (en) * 2004-12-30 2006-07-06 Hon Hai Precision Industry Co., Ltd. Process for manufacturing a reference leak
US20110200450A1 (en) * 2010-02-16 2011-08-18 Edwards Limited Apparatus and method for tuning pump speed

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GB0605360D0 (en) * 2006-03-16 2006-04-26 Dupont Teijin Films Us Ltd Method of manufacture
IT1393996B1 (it) * 2008-09-18 2012-05-17 Univ Degli Studi Genova Dispositivo di fuga di riferimento per la calibrazione delle perdite
IT1400850B1 (it) * 2009-07-08 2013-07-02 Varian Spa Apparecchiatura di analisi gc-ms.
DE102009035745A1 (de) * 2009-08-01 2011-02-17 Christian-Albrechts-Universität Zu Kiel Elektrode für Lithium-Ionen Akkumulatoren
JP5419082B2 (ja) * 2009-08-28 2014-02-19 独立行政法人産業技術総合研究所 標準混合ガスリーク用微小孔フィルターの校正方法及び校正装置
JP5761706B2 (ja) * 2011-01-25 2015-08-12 国立研究開発法人産業技術総合研究所 基準微小ガス流量導入方法
CN102192822B (zh) * 2011-03-10 2012-10-10 安徽皖仪科技股份有限公司 高温石英膜氦质谱漏孔
DE102012219047A1 (de) * 2012-10-18 2014-04-24 Inficon Gmbh Prüfleckvorrichtung zum Anbringen an einer flexiblen Wandung des Prüflings
DE102013215278A1 (de) * 2013-08-02 2015-02-05 Inficon Gmbh Prüfleckvorrichtung mit integriertem Drucksensor
DE102013216450A1 (de) * 2013-08-20 2015-02-26 Inficon Gmbh Pico-Prüfleck
CN105738038B (zh) * 2016-01-29 2018-05-18 合肥工业大学 一种分子流标准漏孔及其制作方法
JP6857179B2 (ja) * 2016-05-31 2021-04-14 株式会社フクダ リークテスト方法およびリークテスト用疑似漏れ器
CN106981432B (zh) * 2017-04-11 2019-04-23 合肥工业大学 一种铜铜键合制作通道型标准漏孔的方法
CN110146426A (zh) * 2019-06-13 2019-08-20 广州西唐机电科技有限公司 检测水蒸气及气体的透过和泄漏量的标准物及其制备方法
CN112284634B (zh) * 2020-10-27 2022-11-01 北京卫星环境工程研究所 一种基于石墨烯的标准漏孔及制备方法

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US2499977A (en) * 1943-11-03 1950-03-07 Gen Electric Method of forming grid-like structures
US3482703A (en) * 1967-11-17 1969-12-09 Brunswick Corp Particulate and biological filters
US3751271A (en) * 1970-05-12 1973-08-07 Toyota Kk Sintered filter having straight holes therethrough
US3680576A (en) * 1970-09-02 1972-08-01 Bendix Corp Bonded metal structure having intricate passages formed therein, and a method of making said structures
US3724825A (en) * 1970-09-24 1973-04-03 Rigips Stempel Gmbh Insert for treating fluids and gases
US3693457A (en) * 1971-02-24 1972-09-26 Battelle Development Corp Source test cascade impactor
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060143895A1 (en) * 2004-12-30 2006-07-06 Hon Hai Precision Industry Co., Ltd. Process for manufacturing a reference leak
US7757371B2 (en) * 2004-12-30 2010-07-20 Tsinghua University Process for manufacturing a reference leak
US20110200450A1 (en) * 2010-02-16 2011-08-18 Edwards Limited Apparatus and method for tuning pump speed
US8657584B2 (en) * 2010-02-16 2014-02-25 Edwards Limited Apparatus and method for tuning pump speed

Also Published As

Publication number Publication date
CN1800801A (zh) 2006-07-12
US20060144120A1 (en) 2006-07-06
JP2006189425A (ja) 2006-07-20
JP4246733B2 (ja) 2009-04-02
CN100462706C (zh) 2009-02-18

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